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Water → Ethanone, 2-(diphenylphosphinothioyl)-1-phenyl-

HRID 1371244
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HRID 1371244 반응식
[C:1]1([PH:7](=[S:14])[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:16][C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:18].[OH-].[K+].O>C(Cl)Cl>[C:19]1([C:17]([CH2:16][P:7](=[S:14])([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[O:18])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 107572-ChloroacetophenoneHCID 14797Potassium HydroxideHCID 178528040HCID 178528040, 화합물

생성물 1

HCID 614971Ethanone, 2-(diphenylphosphinothioyl)-1-phenyl-

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A stirred mixture of diphenylphosphine sulfide (0.218 g, 0.001 mol) and chloroacetophenone (0.216 g, 0.0014 mol) in methylene chloride (4 ml) was cooled to 8–10° C. in an ice-water bath. Small pieces of solid potassium hydroxide (0.196 g, 0.0035 mol) were added while stirring under nitrogen atmosphere. After 45 minute, water (2 ml) was added and the organic layer was separated, washed with more water (2 ml) and dried over sodium sulfate. The solvent was removed under reduced pressure using a rotary evaporator and the oily residue was crystallized from ethyl acetate-hexane mixture to give 0.19 g (56.5%) of star shaped crystals. mp=83–84° C.

후처리

  1. temperaturewas cooled to 8–10° C. in an ice-water bath
  2. customthe organic layer was separated
  3. washwashed with more water (2 ml)
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customa rotary evaporator
  7. customthe oily residue was crystallized from ethyl acetate-hexane mixture
  8. customto give 0.19 g (56.5%) of star

출처 및 근거

ORD 기록
ord-d9125d3c4a3b428e8432974472c5764b
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07157219B2

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